反应详情

温度

92.5 °C

Raney Nickel (6.0 g, in EtOH) is added to a suspension of [4-(6-hydroxy-2-mercapto-pyrimidin-4-ylmethyl)-phenyl]-carbamic acid tert-butyl ester (2.0 g, 5.99 mmol) in MeOH (58 mL), under an argon atmosphere. The resulting mixture is heated to reflux for 2 h (oil bath is pre-heated to 90-95° C.), allowed to cool to rt, filtered through a pad of celite and concentrated in vacuo. The residue is purified by silica gel (160 g) column chromatography (CH2Cl2/MeOH, 95/5, then 90/10) to provide the title compound as a white solid: ES-MS: 302.1 [M+H]+; single peak at tR=6.54 min (System 2); Rf=0.34 (CH2Cl2/MeOH, 90/10).

1. temperatureThe resulting mixture is heated
2. temperatureto reflux for 2 h
3. temperatureto cool to rt
4. filtrationfiltered through a pad of celite
5. concentrationconcentrated in vacuo
6. customThe residue is purified by silica gel (160 g) column chromatography (CH2Cl2/MeOH, 95/5